Full phase analysis of portland clinker by penetrating synchrotron powder diffraction

Fabrication of portland cements commonly depends on X-ray fluorescence (XRF), which measures the elemental compositions. XRF is used to adjust the raw material proportions and to control the process conditions. However, to predict the mechanical strength of the resulting concrete, it is essential to know the phase composition which is, so far, indirectly inferred by the Bogue method. Here, we report a phase analysis of an industrial portland clinker containing six crystalline phases, Ca3SiO5, Ca2SiO4, Ca4Al2Fe2O10, Ca3Al2O6, NaK3(SO4)2, and CaO, by Rietveld refinement of synchrotron X-ray powder diffraction data (lambda = 0.442377 A). Even the minor component, CaO 0.45(2)%, was readily analyzed. We have also carried out a phase study of the same clinker with laboratory X-rays to characterize the changes in the detection limit and errors. Furthermore, by adding a suitable crystalline standard to the same clinker, we have determined the overall amorphous phase content. The procedure established for this state-of-the-art phase analysis shows the high precision that can be achieved by using penetrating X-rays, which is of interest not only in cement chemistry but in other industrially important multiphase systems such as slags, superalloys, or catalysts.